CN106191770A - Porous silicon nitride based sealing coating and preparation method and application - Google Patents
Porous silicon nitride based sealing coating and preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of porous silicon nitride based sealing coating and preparation method and application.Among an embodiment, the method includes: selecting monocrystalline silicon target is negative electrode, magnetron sputtered deposition technology is utilized to prepare silicon nitride hole sealing coating in a nitrogen atmosphere, certain Technology for Heating Processing is used to carry out high temperature sintering subsequently, then hydrophobic modifier is utilized to carry out hydrophobic treatment, thus obtain porous silicon nitride based sealing coating, this hole sealing coating is good with the associativity of nitride porous silicon substrate, and have that compact structure, thickness is controlled, the advantage such as high rigidity, low internal stress, non-nuclear density gauge and high wave, can be applicable to multiple fields.The present invention prepares silicon nitride-based sealing coating by multiple technologies are compound mutually, it is thus achieved that has the silicon nitride-based sealing coating of excellent comprehensive performance, thus can realize the effective protection to nitride porous silicon substrate.
Description
Technical field
The present invention relates to the hole sealing coating of a kind of nitride porous silicon materials, refer more particularly to one and there is the property such as super-hydrophobic, high wave transparent
Silicon nitride-based sealing coating of energy and preparation method and application, belongs to technical field of material surface treatment.
Background technology
Porous silicon nitride becomes heat penetration ripple material because of the advantage such as have that low-k, high-frequency dielectric constant be stable and thermostability is good
One of the study hotspot in material field.Porous silicon nitride can be regarded as the complex of silicon nitride and pore, when the porosity is more than 50%
Time can meet the requirement of low-k.But, the loose structure of silicon nitride also brings while reducing dielectric constant
Adverse influence, as loose structure significantly reduces the mechanical property of silicon nitride, the especially hardness on porous silicon nitride top layer with anti-
Erosion ability；Additionally, the pore on nitride porous silicon materials itself and surface thereof easily adsorbs the aqueous vapor in air, thus affect it
Dielectric properties and heat-proof quality.Therefore, prepare one layer of fine and close hole sealing coating at nitride porous silicon face and both can improve porous nitrogen
The erosion resistance of SiClx, can play again the impact of isolation aqueous vapor, and the application for porous materials such as porous silicon nitrides has weight
The construction value wanted.
Chemical vapour deposition technique (CVD) and sol-gal process is currently mainly used to prepare the hole sealing coating of porous silicon nitride.Wherein
CVD be directly nitride porous silicon face deposition compact Si3N4Ceramic coating, the compact silicon nitride coating deposited has
There are the thermal coefficient of expansion consistent with matrix, high mechanical strength, low-k and dielectric loss.But, in CVD plated film
Harmful gas need to be used, and CVD cavity is not easy to prepare big sample, limits the application of this technology.Sol-gel process is
By preparing oxide sol, it is fired into vitreous coating subsequently and sealing of hole.This technology has the advantages such as simple, easy expansion,
But coating often can cause coating to be prone in heating/cooling occur damage to lose efficacy with the thermal expansion coefficient difference of matrix, and aoxidizes
The existence of thing improves the dielectric constant of hole sealing coating.
Summary of the invention
Present invention is primarily targeted at and provide a kind of that have performances such as top layer wave hydrophobic, high and low stress and quality to cause
Close porous silicon nitride based sealing coating and preparation method thereof.
Another object of the present invention is to provide the purposes of described porous silicon nitride based sealing coating.
For realizing aforementioned invention purpose, the technical solution used in the present invention includes:
A kind of preparation method of porous silicon nitride based sealing coating, comprising:
(1) nitride porous silicon substrate is cleaned with plasma sputtering,
(2) use monocrystalline silicon target as negative electrode, and using noble gas and nitrogen as working gas, existed by magnetron sputtering technique
Described deposited on substrates silicon nitride-based sealing coating, cools down afterwards；
(3) base material after step (2) processes is carried out heat treatment, be cooled to room temperature；
(4) with hydrophobic modifier, the silicon nitride-based sealing coating after step (3) processes is carried out hydrophobic treatment.
As one of preferred embodiment, step (1) may include that and nitride porous silicon substrate is placed in magnetron sputtering vapor deposition
In system, utilizing argon plasma to carry out sputter clean, wherein argon gas flow is 80～150sccm, bias as-300V～
700V, the process time is 10min～30min.
As one of preferred embodiment, step (2) may include that employing magnetron sputtering deposition technique, using monocrystalline silicon target as
Negative electrode, argon and nitrogen are as working gas, and to control power be 600W～1200W, bias as-120V, argon stream
Amount is 50～100sccm, and nitrogen flow is 120～180sccm, and the magnetron sputtering deposition time is 5h～60h, thus through step
(1) the porous silicon nitride deposited on substrates silicon nitride-based sealing coating after processing.
Further, step (2) can also include: after magnetron sputtering deposition silicon nitride-based sealing coating reaches to set thickness,
Stop plated film, and continue to be passed through nitrogen and argon in the plated film chamber of magnetron sputtering vapor depositing system, until in plated film chamber
Temperature be down to less than 100 DEG C, take out with the base material of silicon nitride-based sealing coating.
As one of preferred embodiment, the heat treatment temperature used in step (3) is 600～1500 DEG C, the time be 0.5h～
5h, atmosphere is air atmosphere or nitrogen protection atmosphere.
Further, step (4) including: the base material after step (3) processes be impregnated in the hydrolysis containing hydrophobic modifier
In liquid, soaking at room temperature 5～20h, continues to soak 2～6h at 50～80 DEG C afterwards, then takes out, formed and dredge on described base material
Water silicon nitride hole sealing coating.
Further, described hydrophobic modifier is at least selected from silicon fluoride, such as preferably from ten difluoro heptyl propyl trimethoxy silicon
Alkane or 17 fluorine decyl trimethoxy silanes, but it is not limited to this.
The porous silicon nitride based sealing coating prepared by preceding method, it has main by Si3N4And Si2N2O phase spherical particle group
The compact texture become.
Further, the hardness of described hole sealing coating is 5～15GPa, is more than 40N with the bond strength of nitride porous silicon substrate,
And there is the thermal coefficient of expansion consistent with described nitride porous silicon substrate and wave.
Further, described hole sealing coating is 100～130 ° with the contact angle of water.
Further, the thickness of described hole sealing coating can adjust, such as according to the sealing of hole demand of different porosities porous silicon nitride
Can be 5～70 μm.
Among an application scheme, present invention also offers a kind of silicon nitride-based material, it comprises is prepared by any one method aforementioned
Hole sealing coating.
Among an application scheme, present invention also offers a kind of device, it comprises nitride porous silicon substrate, described nitride porous
Described hole sealing coating is distributed on silicon substrate.
Compared with prior art, the present invention at least has the advantage that
(1) hole sealing coating that the present invention provides is mainly by Si3N4And Si2N2O phase spherical particle is formed, the structure of hole sealing coating
Fine and close and have consistent thermal coefficient of expansion with nitride porous silicon substrate, this hole sealing coating also has high mechanical strength in addition, low
Dielectric constant, dielectric loss and high wave, such as, hardness is 5～15GPa, and scratching instrument is measured bond strength and is more than 40N,
Before and after plated film, the change in dielectric constant of porous silicon nitride substrate sample is not more than 5%；
(2) especially preferred, modified by the hole sealing coating of the present invention being carried out surface hydrophobicity, its super-hydrophobicity can be given,
Coating is made to avoid absorbing steam and more erosion resistance in placement process；
(3) sample size is limited little by the hole sealing coating preparation technology that the present invention provides, and can prepare large-sized sample.
Accompanying drawing explanation
Fig. 1 is the surface water droplet state diagram of silicon nitride-based sealing coating after embodiment 1 hydrophobically modified processes；
Fig. 2 is the X-ray diffractogram of embodiment 1 silicon nitride-based sealing coating；
Fig. 3 a-3b is respectively surface topography and the Cross Section Morphology figure of embodiment 1 silicon nitride-based sealing coating.
Detailed description of the invention
In view of many defects of prior art, inventor, through studying for a long period of time and putting into practice in a large number, is proposed the technology of the present invention
Scheme, it will be as it was noted above, it more specifically will be illustrated by the applicant in conjunction with ensuing disclosure.
One aspect of the present invention provides a kind of hydrophobic silicon nitride hole sealing coating, and it is mainly by Si3N4And Si2N2O phase composition,
Its associativity with nitride porous silicon substrate is good, and have that compact structure, thickness is controlled, high rigidity, low internal stress, without grand
The advantage such as defect and high wave of sight.
Among some more preferred embodiment, the thickness of described coating can be 5～70 μm, many to meet different porosities
The sealing of hole demand of hole silicon nitride, and coating is 100～130 ° for the contact angle of water.
Another aspect of the present invention provides a kind of method preparing described hydrophobic silicon nitride hole sealing coating, and it is mainly by choosing
Selecting monocrystalline silicon target is negative electrode, utilizes DC reactive sputtering technology to prepare silicon nitride hole sealing coating in a nitrogen atmosphere, uses one subsequently
Fixed Technology for Heating Processing carries out high temperature sintering, then utilizes hydrophobic modifier to carry out hydrophobic treatment, thus acquisition has hydrophobic, high
The compact silicon nitride base coating of wave transparent characteristic.
In a preferred embodiment, the preparation method of a kind of hydrophobic silicon nitride hole sealing coating may comprise steps of:
(1) plasma sputtering cleans base material, by nitride porous silicon substrate as in magnetron sputtering vapor depositing system, utilizes argon
Plasma carries out sputter clean, and argon gas flow is 80-150sccm, biases as-300V to 700V, and the process time is
10min to 30min；
(2) magnetron sputtering deposition silicon nitride-based sealing coating, monocrystalline silicon target is negative electrode, control power be 600W extremely
1200W, biases as-120V, and it is argon, nitrogen that plated film cavity is passed through gas, and wherein argon flow amount is 50-100sccm, nitrogen
Flow is 120-180sccm, utilizes reaction magnetocontrol sputtering technology to prepare silicon nitride-based sealing coating；Process basis of time coating layer thickness
For 5h to 60h；
(3) to be coated to (i.e. silicon nitride-based sealing coating) reach suitable thickness, stop plated film, continue to be passed through nitrogen in cavity
Gas and argon, until cavity inner temperature is down to less than 100 DEG C, take out the sample after plated film.
(4) heat treatment of silicon nitride-based sealing coating, puts in heating furnace by the sample after plated film, carries out heat treatment, heat treatment
Time is 0.5h-5h, and heat-treating atmosphere is air, nitrogen, terminates rear stove and is cooled to room temperature.
(5) nitrogenize the hydrophobically modified of silica-based coating, select hydrophobic modifier that heat treating silicon nitride based sealing coating is carried out hydrophobic place
Reason, immerses sample in the hydrolyzed solution containing hydrophobic modifier, soaking at room temperature 5-20h, and then 50-80 DEG C is continued to soak 2-6h,
Process takes out sample after terminating, and i.e. obtains hydrophobic silicon nitride hole sealing coating.
Further, in step (4), by heat treatment, the elemental silicon in coating can be changed into silicon oxide, it is to avoid
Coating causes the increase of the dielectric constant of material owing to elemental silicon exists, and reduces the thermal stress of thin film, the painting of raising
The service safety of layer.
Further, described hydrophobic modifier is preferably silicon fluoride, such as ten difluoro heptyl propyl trimethoxy silicanes or ten
Seven fluorine decyl trimethoxy silanes, wherein after the siloxanes generation hydrolysis in silicon fluoride structure, hydroxyl with silicon nitride surface is sent out
Raw bonding, thus form fluorine-containing coating at coating surface so that coating has ultra-hydrophobicity, and the steam in air is in coating
The water droplet that surface is formed can be with roller ball form landing, without sprawling at coating surface, thus further improves the resistance to punching of coating
The ability of erosion.
The present invention prepares silicon nitride-based sealing coating by multiple technologies are compound mutually, it is thus achieved that have wave transparent characteristic hydrophobic, high many
Hole silicon nitride-based sealing coating, it is possible to achieve the effective protection to nitride porous silicon substrate, and substantially without silica-based to nitride porous
The performance of material causes damage.
Embodiment 1: this high wave transparent silicon nitride-based sealing coating, by the Si that nitride porous silicon substrate, thickness are 33.5 μm3N4With
Si2N2The spherical particle dense coating of O phase is formed, coating contact angle 116.3 °.
The preparation technology of this high wave transparent silicon nitride coating follows the steps below: (1) plasma sputtering cleans base material: first will
Nitride porous silicon substrate after over cleaning is put in magnetron sputtering apparatus vacuum cavity, carries out argon plasma sputter clean, argon
Gas flow is 120sccm, biases as-500V, and the process time is 30min；(2) the silica-based coating of magnetron sputtering deposition nitridation:
Monocrystalline silicon target is negative electrode, and vacuum chamber pressure is 8.0*10-1Pa, working gas is argon, nitrogen, flow be respectively 60sccm,
180sccm, controlling DC source power is 1000W, and substrate bias is-120V, and the process time is 9h；(3) silica-based envelope is nitrogenized
The heat treatment of hole coating: put in heat-treatment furnace by reaction magnetocontrol sputtering plated film sample, selecting heat treatment temperature is 1200 DEG C, rises
Temperature speed is 5 DEG C/min, and 1200 DEG C of insulation 0.5h, air atmosphere, stove is cooled to room temperature；(4) silicon nitride-based sealing coating is hydrophobic
Modification: select ten difluoros heptyl propyl trimethoxy silicane (G502) to carry out hydrophobic to heat treating silicon nitride based sealing coating
Processing, solution is 30ml ethanol, 5ml deionized water, 3ml G502, and sample is immersed molten by supersound process 2h subsequently after mixing
Liquid, soak time is 5h, and then 70 DEG C are continued to soak 6h, and process takes out sample after terminating, and i.e. obtains hydrophobic nitridation silica-based
Hole sealing coating, contact angle is 116.3 °.
Table 1 is embodiment 1 silicon nitride hole sealing coating (silicon nitride hole sealing coating face) and its porous substrate material (untreated face)
Dielectric constant, the silicon nitride-based sealing coating of Combined Processing has low dielectric constant and dielectric loss as can be seen from Table 1.
Table 1 embodiment 1 silicon nitride hole sealing coating and the dielectric constant on perforated substrate surface
Embodiment 2: this high wave transparent silicon nitride-based sealing coating, spherical by the SiN phase that nitride porous silicon substrate, thickness are 12 μm
Granule dense coating is formed, coating contact angle 125 °.
The preparation technology of this high wave transparent silicon nitride coating follows the steps below: (1) plasma sputtering cleans base material: first will
Nitride porous silicon substrate after over cleaning is put in magnetron sputtering apparatus vacuum cavity, carries out argon plasma sputter clean, argon
Gas flow is 120sccm, biases as-500V, and the process time is 30min；(2) the silica-based coating of magnetron sputtering deposition nitridation:
Monocrystalline silicon target is negative electrode, and vacuum chamber pressure is 8.0*10-1Pa, working gas is argon, nitrogen, flow be respectively 60sccm,
180sccm, controlling DC source power is 1000W, and substrate bias is-120V, and the process time is 9h；(3) nitrogenize silica-based
The heat treatment of hole sealing coating: reaction magnetocontrol sputtering plated film sample is put in heat-treatment furnace, selecting heat treatment temperature is 600 DEG C,
Heating rate is 5 DEG C/min, is incubated 2h, and air atmosphere, stove is cooled to room temperature；(4) hydrophobically modified of silicon nitride-based sealing coating
Process: selecting 17 fluorine decyl trimethoxy silanes that heat treating silicon nitride based sealing coating is carried out hydrophobic treatment, solution is 30ml
Ethanol, 5ml deionized water, supersound process 2h after mixing, subsequently sample is immersed solution, soak time is 5h, then 70 DEG C
Continuing to soak 6h, process takes out sample after terminating, and i.e. obtains silicon nitride-based sealing coating.
Table 2 is embodiment 2 silicon nitride hole sealing coating (silicon nitride hole sealing coating face) and its porous substrate material (untreated face)
Dielectric constant, the silicon nitride-based sealing coating after Combined Processing has low dielectric constant and dielectric and damages as can be seen from Table 2
Consumption.
Table 2 embodiment 2 silicon nitride hole sealing coating and the dielectric constant on perforated substrate surface
Embodiment 3: this high wave transparent silicon nitride-based sealing coating is by the Si that nitride porous silicon substrate, thickness are 33.5 μm3N4With
Si2N2O spherical particle dense coating is formed.
The preparation technology of this high wave transparent silicon nitride coating follows the steps below: (1) plasma sputtering cleans base material: first will
Nitride porous silicon substrate after over cleaning is put in magnetron sputtering apparatus vacuum cavity, carries out argon plasma sputter clean, argon
Gas flow is 120sccm, biases as-500V, and the process time is 30min；(2) the silica-based coating of magnetron sputtering deposition nitridation:
Monocrystalline silicon target is negative electrode, and vacuum chamber pressure is 8.0*10-1Pa, working gas is argon, nitrogen, flow be respectively 60sccm,
180sccm, controlling DC source power is 1000W, and substrate bias is-120V, and the process time is 25h；(3) nitrogenize silica-based
The heat treatment of hole sealing coating: reaction magnetocontrol sputtering plated film sample is put in heat-treatment furnace, selecting heat treatment temperature is 1200 DEG C,
Heating rate is 5 DEG C/min, and 1200 DEG C of insulation 60min, air atmosphere, stove is cooled to room temperature；(4) silicon nitride-based sealing coating
Hydrophobically modified processes: select ten difluoros heptyl propyl trimethoxy silicane (G502) to carry out heat treating silicon nitride based sealing coating
Hydrophobic treatment, solution is 30ml ethanol, 5ml deionized water, 3ml G502, supersound process 2h after mixing, is soaked by sample subsequently
Entering solution, soak time is 5h, and then 70 DEG C are continued to soak 6h, and process takes out sample after terminating, and i.e. obtains nitrogenizing silica-based envelope
Hole coating, takes out sample, it is thus achieved that have the silicon nitride-based sealing coating material of high wave transparent characteristic.
Embodiment 4: this high wave transparent silicon nitride-based sealing coating is by the Si that nitride porous silicon substrate, thickness are 65 μm3N4And Si2N2O
Spherical particle dense coating is formed.
The preparation technology of this high wave transparent silicon nitride coating can follow the steps below: (1) plasma sputtering cleans base material: first
First the nitride porous silicon substrate after over cleaning is put in magnetron sputtering apparatus vacuum cavity, carries out argon plasma sputter clean,
Argon gas flow is 120sccm, biases as-500V, and the process time is 30min；(2) magnetron sputtering deposition nitrogenizes silica-based painting
Layer: monocrystalline silicon target is negative electrode, and vacuum chamber pressure is 8.0*10-1Pa, working gas is argon, nitrogen, flow be respectively 60sccm,
180sccm, controlling DC source power is 1000W, and substrate bias be-120V, plated film for running 10h, in stop 1h, meter 5
Individual circulation, altogether 50h；(3) heat treatment of silicon nitride-based sealing coating: reaction magnetocontrol sputtering plated film sample is put into heat-treatment furnace
In, selecting heat treatment temperature is 1200 DEG C, and heating rate is 5 DEG C/min, and 1200 DEG C of insulation 60min, air atmosphere, stove is cooled to
Room temperature；(4) hydrophobically modified of silicon nitride-based sealing coating processes: select ten difluoros heptyl propyl trimethoxy silicane (G502)
Heat treating silicon nitride based sealing coating is carried out hydrophobic treatment, and solution is 30ml ethanol, 5ml deionized water, 3ml G502, mixed
Supersound process 2h after conjunction, immerses solution subsequently by sample, and soak time is 5h, and then 70 DEG C are continued to soak 6h, and process terminates
Rear taking-up sample, i.e. obtains silicon nitride-based sealing coating.
Should be appreciated that above-described embodiment is only technology design and the feature of the explanation present invention, its object is to allow and be familiar with technique
Personage will appreciate that present disclosure and implement according to this, can not limit the scope of the invention with this.All according to this
The equivalence that bright spirit is made changes or modifies, and all should contain within protection scope of the present invention.
Claims (9)
1. the preparation method of a porous silicon nitride based sealing coating, it is characterised in that including:
(1) nitride porous silicon substrate is cleaned with plasma sputtering；
(2) use monocrystalline silicon target as negative electrode, and using noble gas and nitrogen as working gas, existed by magnetron sputtering technique
Described deposited on substrates silicon nitride-based sealing coating, cools down afterwards；
(3) by the base material after step (2) processes is carried out heat treatment, it is cooled to room temperature；
(4) with hydrophobic modifier, the silicon nitride-based sealing coating after step (3) processes is carried out hydrophobic treatment.
The preparation method of porous silicon nitride based sealing coating the most according to claim 1, it is characterised in that step (1) is wrapped
Include: nitride porous silicon substrate is placed in magnetron sputtering vapor depositing system, utilize argon plasma to carry out sputter clean, wherein
Argon gas flow is 80～150sccm, biases as-300V～700V, and the process time is 10min～30min.
The preparation method of porous silicon nitride based sealing coating the most according to claim 1, it is characterised in that step (2) is wrapped
Include: use magnetron sputtering deposition technique, using monocrystalline silicon target as negative electrode, argon and nitrogen as working gas, and control power supply
Power is 600W～1200W, biases as-120V, and argon flow amount is 50～100sccm, and nitrogen flow is 120～180sccm,
The magnetron sputtering deposition time is 5h～60h, thus the porous silicon nitride deposited on substrates nitridation after processing through step (1) is silica-based
Hole sealing coating.
The preparation method of porous silicon nitride based sealing coating the most according to claim 3, it is characterised in that step (2) is wrapped
Include: after magnetron sputtering deposition silicon nitride-based sealing coating reaches to set thickness, stop plated film, and continue to magnetron sputtering vapor
Be passed through nitrogen and argon in the plated film chamber of depositing system, until the temperature in plated film chamber is down to less than 100 DEG C, take out with
The base material of silicon nitride-based sealing coating.
5. according to the preparation method of porous silicon nitride based sealing coating according to any one of claim 1,4, it is characterised in that
The heat treatment temperature used in step (3) is 600～1500 DEG C, and the time is 0.5h～5h, and atmosphere is air atmosphere or nitrogen guarantor
Protect atmosphere.
The preparation method of porous silicon nitride based sealing coating the most according to claim 1, it is characterised in that step (4)
Including: the base material after step (3) processes be impregnated in the hydrolyzed solution containing hydrophobic modifier, soaking at room temperature 5～20h,
Continue to soak 2～6h at 50～80 DEG C afterwards, then take out, on described base material, form hydrophobic silicon nitride hole sealing coating.
7. according to the preparation method of the porous silicon nitride based sealing coating according to any one of claim 1,6, it is characterised in that
Described hydrophobic modifier is at least selected from silicon fluoride, and described silicon fluoride includes ten difluoro heptyl propyl trimethoxy silicane or 17 fluorine
Decyl trimethoxy silane.
8. the porous silicon nitride based sealing coating prepared by method according to any one of claim 1-7, it is characterised in that described envelope
Hole coating has main by Si3N4And Si2N2The compact texture of O spherical particle composition, and the hardness of described hole sealing coating is
5～15GPa, it is more than 40N with the bond strength of nitride porous silicon substrate, and there is the heat consistent with described nitride porous silicon substrate
The coefficient of expansion and wave, the most described hole sealing coating is 100～130 ° with the contact angle of water.
9. a silicon nitride-based material, it is characterised in that comprise the sealing of hole prepared by method according to any one of claim 1-7 and be coated with
Layer.
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| CN116180075A (en) * | 2023-02-17 | 2023-05-30 | 西南交通大学 | Preparation method of low-stress strong-bonding high-temperature insulating coating |
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